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Method for preparing m-aminophenol by catalytic hydrolysis of m-phenylenediamine

A technology of m-aminophenol and m-phenylenediamine, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of amino hydroxy compounds, etc., can solve problems such as no cost advantage, and achieve high product yield and good product quality. , the effect of low cost of raw materials

Inactive Publication Date: 2009-09-23
台州市经纬化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0019] The method uses resorcinol as a raw material and ammonia under high temperature and high pressure to generate m-aminophenol through ammonolysis, which has certain advantages due to less three wastes. In the 1980s, Japan's Mitsui and Sumitomo companies respectively built production devices and put them into production. However, the price of resorcinol is close to that of m-aminophenol, and this production route does not have a cost advantage

Method used

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  • Method for preparing m-aminophenol by catalytic hydrolysis of m-phenylenediamine
  • Method for preparing m-aminophenol by catalytic hydrolysis of m-phenylenediamine
  • Method for preparing m-aminophenol by catalytic hydrolysis of m-phenylenediamine

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Effect test

Embodiment 1

[0033] In a 250ml autoclave made of zirconium, add 4.5g of m-phenylenediamine, 50ml of water, and 6.6ml of 37% hydrochloric acid, seal the autoclave, and replace it with nitrogen 2 to 3 times. Heat up to 205°C. At this time, the pressure in the kettle is 1.9 MPa. Keep the temperature for 4 hours, cool down to 30°C, release the pressure in the kettle, pour the contents of the kettle into a separatory funnel, and use 3*20ml methyl The isobutyl ketone was extracted three times to combine the organic phase, the organic phase was demethylated by methyl isobutyl ketone, and the resorcinol with a purity of 99% was obtained by vacuum distillation. The previous aqueous phase was adjusted to pH 14 with sodium hydroxide, extracted three times with 3*20ml methyl isobutyl ketone, the organic phase was combined, back-extracted with 20ml 5% hydrochloric acid, the organic phase was combined, and methyl isobutyl ketone was obtained after phase separation The ketone is reused to obtain the m-ph...

Embodiment 2

[0035] The basic preparation process is the same as in Example 1, the difference is that 4.5g of m-phenylenediamine, 50ml of water, and 6.6ml of 37% hydrochloric acid are respectively added to the autoclave made of zirconium, and the temperature is raised to 180°C. At this time, the pressure in the autoclave is 0.9MPa , keep the temperature for 10 hours, and cool down. The sample was analyzed by high-pressure liquid chromatography, and the conversion rate of m-phenylenediamine was 57%, and the selectivity of m-aminophenol was 91%.

Embodiment 3

[0037] The basic preparation process is the same as in Example 1, the difference is that 4.5g of m-phenylenediamine, 50ml of water, and 7.6ml of 37% hydrochloric acid are respectively added to the autoclave made of zirconium, and the temperature is raised to 190°C. At this time, the pressure in the autoclave is 1.2MPa , keep the temperature for 9 hours, and cool down. The sample was analyzed by high-pressure liquid chromatography, and the conversion rate of m-phenylenediamine was 51%, and the selectivity of m-aminophenol was 95%.

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Abstract

The invention provides a method for preparing m-aminophenol by the catalytic hydrolysis of m-phenylenediamine, which comprises the following steps: under the condition of the existence of inorganic acid catalysts, m-phenylenediamine is hydrolyzed at the temperature of 180 DEG C to 230 DEG C and the pressure of 0.9 to 3.0 MPa for 2 to 10 hours; a solvent is adopted to extract hydrolysis products to respectively obtain m-dihydroxybenzene extraction liquid, m-phenylenediamine extraction liquid and m-aminophenol extraction liquid according to different pH values, and then the m-phenylenediamine extraction liquid is processed to be used as raw material for hydrolysis next time; the m-aminophenol extraction liquid is processed by vacuum distillation after being processed by exsolution, and then active carbon is decolourized and recrystallized to obtain m-aminophenol whose purity is more than 99 percent; and the m-dihydroxybenzene extraction liquid is processed by vacuum distillation after being processed by exsolution to obtain the m-dihydroxybenzene whose purity is 99 percent. The method for preparing m-aminophenol by catalytic hydrolysis of m-phenylenediamine is adopted, and proper technological conditions are controlled in the reaction process. The method has the advantages of low cost of raw material and high product yield.

Description

technical field [0001] The invention relates to a method for preparing m-aminophenol, in particular to a method for preparing m-aminophenol by catalytic hydrolysis of m-phenylenediamine. It belongs to the field of organic synthesis. Background technique [0002] m-Aminophenol is an important intermediate of pesticides, medicines, dyes and functional materials. It is widely used in pesticides, medicines, dyes and other industries. It is also used in the production of antioxidants, stabilizers, developers and catalysts for organic chemical reactions. Wait. [0003] The traditional method of producing m-aminophenol is to use nitrobenzene as a raw material, which is sulfonated by sulfur trioxide to generate m-nitrobenzenesulfonic acid, and 3,3-dinitrodiphenyl sulfone is produced as a by-product. [0004] [0005] side effects [0006] [0007] The m-nitrobenzenesulfonic acid is neutralized with sodium hydroxide to form sodium m-nitrobenzenesulfonate, and the by-product ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/78C07C213/00
Inventor 李付刚邢小蓬白雪松李显龙李文骁余昌富闫士杰
Owner 台州市经纬化工有限公司
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